WO2020202718A1 - Plated material and method for manufacturing same - Google Patents

Plated material and method for manufacturing same Download PDF

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Publication number
WO2020202718A1
WO2020202718A1 PCT/JP2020/002032 JP2020002032W WO2020202718A1 WO 2020202718 A1 WO2020202718 A1 WO 2020202718A1 JP 2020002032 W JP2020002032 W JP 2020002032W WO 2020202718 A1 WO2020202718 A1 WO 2020202718A1
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WO
WIPO (PCT)
Prior art keywords
plating
plating film
film
tin
silver
Prior art date
Application number
PCT/JP2020/002032
Other languages
French (fr)
Japanese (ja)
Inventor
悠太郎 平井
健太郎 荒井
俊祐 足達
Original Assignee
Ｄｏｗａメタルテック株式会社
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Ｄｏｗａメタルテック株式会社 filed Critical Ｄｏｗａメタルテック株式会社
Priority to CN202080025302.8A priority Critical patent/CN113677831B/en
Priority to US17/435,746 priority patent/US11898263B2/en
Priority to EP20784961.3A priority patent/EP3919656A4/en
Priority to MX2021011866A priority patent/MX2021011866A/en
Publication of WO2020202718A1 publication Critical patent/WO2020202718A1/en

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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00—Electroplating characterised by the article coated
    • C25D7/06—Wires; Strips; Foils
    • C25D7/0614—Strips or foils
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/30—Electroplating: Baths therefor from solutions of tin
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/46—Electroplating: Baths therefor from solutions of silver
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/011—Electroplating using electromagnetic wave irradiation
    • C25D5/013—Wavelengths other than ultraviolet [UV], visible or infrared [IR], e.g. X-rays or microwaves
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/02—Electroplating of selected surface areas
    • C25D5/022—Electroplating of selected surface areas using masking means
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/10—Electroplating with more than one layer of the same or of different metals
    • C25D5/12—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/48—After-treatment of electroplated surfaces
    • C25D5/50—After-treatment of electroplated surfaces by heat-treatment
    • C25D5/505—After-treatment of electroplated surfaces by heat-treatment of electroplated tin coatings, e.g. by melting
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/60—Electroplating characterised by the structure or texture of the layers
    • C25D5/625—Discontinuous layers, e.g. microcracked layers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
    • H01H1/00—Contacts
    • H01H1/02—Contacts characterised by the material thereof
    • H01H1/021—Composite material
    • H01H1/025—Composite material having copper as the basic material
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/34—Pretreatment of metallic surfaces to be electroplated
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01R—ELECTRICALLY-CONDUCTIVE CONNECTIONS; STRUCTURAL ASSOCIATIONS OF A PLURALITY OF MUTUALLY-INSULATED ELECTRICAL CONNECTING ELEMENTS; COUPLING DEVICES; CURRENT COLLECTORS
    • H01R13/00—Details of coupling devices of the kinds covered by groups H01R12/70 or H01R24/00 - H01R33/00
    • H01R13/02—Contact members
    • H01R13/03—Contact members characterised by the material, e.g. plating, or coating materials

Definitions

  • the present invention relates to a plating material and a method for manufacturing the same, and more particularly to a plating material used as a material for contacts and terminal parts such as connectors, switches, and relays used for in-vehicle and consumer electrical wiring, and a method for manufacturing the same. ..
  • a relatively inexpensive base material such as copper or copper alloy or stainless steel, which has excellent corrosion resistance and mechanical properties, has electrical properties and solderability.
  • Plating materials plated with tin, silver, gold, etc. are used, depending on the required properties.
  • a plating material in which a base layer made of nickel is formed between these platings and the base material is also used.
  • a tin-plated material obtained by tin-plating a base material such as copper or a copper alloy or stainless steel is inexpensive, but inferior in corrosion resistance in a high temperature environment. Further, the gold-plated material obtained by subjecting these base materials to gold plating has excellent corrosion resistance and high reliability, but the cost is high. On the other hand, the silver-plated material obtained by silver-plating these base materials is cheaper than the gold-plated material and has excellent corrosion resistance as compared with the tin-plated material.
  • the part where the male terminal and the female terminal are fitted is plated with gold or silver, and the part where the electric wire is crimped (the crimping part) is inexpensively deformed.
  • a plating material with glossy tin plating or matte tin plating, which is easy to use, may be used.
  • tin plating is generally performed by electroplating, and in order to alleviate the internal stress of the tin plating film and suppress the generation of whiskers, reflow treatment (after melting the tin plating by heating) is performed after electroplating. Processing to solidify) is being performed.
  • reflow treatment is performed after tin plating in this way, a part of tin diffuses into the material and the base component to form a compound layer, and a tin or tin alloy layer is formed on the compound layer.
  • a plating material in which the part where an electric wire made of aluminum or an aluminum alloy is crimped is tin-plated has a high resistance value. Therefore, in order to suppress an increase in the resistance value, a reflow treatment is performed after tin plating. Need to be applied.
  • a nickel base plating layer is formed by electroplating on one surface of a plate-shaped metal member made of copper or a copper alloy, and a silver plating layer is formed on the base plating layer by electroplating.
  • a tin-plated layer is formed on the other surface of the plate-shaped metal member by direct electroplating without a base, and then reflowed by heating to 400 to 800 ° C. in a low oxygen concentration atmosphere with an oxygen concentration of 200 ppm or less to perform tin plating. It is known that a tin-copper metal-to-metal compound is formed between a plate-shaped metal member and a tin-plated layer by melting the layer (see, for example, Patent Document 1).
  • At least a part of the reflow tin plating layer and the reaction layer is completely peeled off from the metal base material in which the reflow tin plating layer is formed at least partially and the reaction layer is formed at the interface with the reflow tin plating layer. It is known that at least a part of the region where the reflow tin plating layer and the reaction layer are completely peeled off is subjected to a nickel plating treatment to form a nickel plating layer, and at least a part of this nickel plating layer is subjected to a tin plating treatment. (See, for example, Patent Document 2).
  • JP-A-2002-134361 (paragraph number 0033)
  • International Publication WO2015 / 092979 (paragraph number 0011)
  • the plating material used as a material for terminal parts such as connectors is plated with gold plating (excellent oxidation resistance) at the fitting part, tin plating at the crimping part, and then reflow processing.
  • gold plating excellent oxidation resistance
  • the contact resistance hardly increases even after heating by the reflow treatment.
  • the plating material used as the material for terminal parts such as connectors is silver-plated (cheaper than gold plating) on the fitting part, tin-plated on the crimped part, and then reflowed.
  • the contact resistance of the silver plating film increases after heating by the reflow treatment and the surface of the silver plating film is discolored.
  • Patent Document 1 requires equipment for heating in a low oxygen concentration atmosphere, which increases the manufacturing cost.
  • the contact resistance of the silver plating layer increases and the surface of the silver plating layer becomes high because the silver plating layer and the tin plating layer coexist and are heated at a high temperature. There is a risk of discoloration.
  • Patent Document 2 requires a step of completely peeling off at least a part of the reflow tin plating layer and the reaction layer, which increases the manufacturing cost.
  • the reflow tin plating layer and the reaction layer may be peeled off more than necessary when they are dissolved in a chemical solution and peeled off.
  • the present invention reflows a plating material having a silver-plated film formed on a part of the surface and a tin-plated film formed on the other part, and then silver-plated. It is an object of the present invention to provide an inexpensive plating material and a method for producing the same, which can prevent an increase in contact resistance of the film and discoloration of the surface.
  • the present inventors formed a nickel-plated film on the surface of a base material made of copper or a copper alloy, and formed a silver-plated film on a part of the surface of the nickel-plated film.
  • a plating material in which a silver plating film and a tin plating film are formed on the surface of the nickel plating film on the base material is formed by forming the tin plating film on a part of the other part of the surface of the nickel plating film.
  • this plating material After the production, the surface of this plating material is irradiated with infrared rays and heated to reflow the tin plating film, and if the tin plating film is made into a reflow tin plating layer, the tin plating film is reflowed and then silver.
  • a plating material can be manufactured at low cost, which can prevent an increase in the contact resistance of the plating film and discoloration of the surface, and have completed the present invention.
  • a nickel plating film is formed on the surface of a base material made of copper or a copper alloy, a silver plating film is formed on a part of the surface of the nickel plating film, and nickel plating is performed.
  • a plating material in which a silver-plated film and a tin-plated film are formed on the surface of the nickel-plated film on the base material is produced, and then this plating is performed.
  • the tin-plated film is reflowed to form a reflowed tin-plated layer.
  • this method for producing a plating material it is preferable to preheat a plating material in which a silver plating film and a tin plating film are formed on the surface of the nickel plating film before irradiation with infrared rays so that the tin plating film does not melt. .. Further, it is preferable that infrared irradiation is performed by an infrared lamp. Further, it is preferable that a part of the surface of the nickel plating film and a part of the other part of the surface of the nickel plating film are separated from each other.
  • a tin plating film after forming a silver plating film.
  • a nickel plating layer is formed on the surface of a base material made of copper or a copper alloy, a silver plating layer is formed on a part of the surface of the nickel plating layer, and a nickel plating film is formed.
  • a reflow tin plating layer is formed on a part of the other portion of the surface of the silver plating layer, and the contact resistance of the surface of the silver plating layer is 1 m ⁇ or less.
  • the silver plating layer and the tin plating layer formed on the surface of the nickel plating layer are separated from each other.
  • the contact resistance of the silver plating film is increased and the surface is discolored. It is possible to manufacture an inexpensive plating material that can prevent the above-mentioned problems at low cost.
  • FIG. 1A is a sectional view taken along line IIA-IIA of FIG. 1A.
  • FIG. 1B is a sectional view taken along line IIB-IIB of FIG. 1B.
  • FIG. 1C is a sectional view taken along line IIC-IIC of FIG. 1C.
  • FIG. 3 is a cross-sectional view taken along line IID-IID of FIG.
  • FIG. 1D It is a cross-sectional view taken along the line IIE-IIE of FIG. 1E.
  • FIG. 2 is a sectional view taken along line IIF-IIF of FIG. 1F.
  • FIG. 5 is a cross-sectional view taken along the line IIG-IIG of FIG.
  • FIG. 2 is a sectional view taken along line IIH-IIG of FIG. 1H.
  • FIG. 2 is a sectional view taken along line IIJ-IIJ of FIG. 1J.
  • a base material 10 made of copper or a copper alloy is prepared.
  • the base material 10 includes pure copper-based base materials such as oxygen-free copper and tough pitch copper, brass, phosphorous bronze, Cu-Ni-Si-based alloys, Cu-Fe-P-based alloys, and Cu-Ni-Sn-P-based base materials.
  • a base material made of a copper alloy such as an alloy can be used.
  • the shape of the base material 10 may be a strip-shaped individual piece, but from the viewpoint of productivity (a plating material can be manufactured by a reel-to-reel type continuous plating line), a strip material is used. preferable.
  • a nickel plating film 12 is formed as a base plating film on substantially the entire surface (rolled surface) of the base material 10.
  • the nickel plating film may be formed by either electroplating or electroless plating, but it is preferably performed by electroplating from the viewpoint of productivity and cost.
  • a mask member 14 is arranged (for example, a masking tape is attached or a resist mask is formed) on a portion other than a part of the surface of the nickel plating film 12, and that portion is formed.
  • a part of the surface of the nickel plating film 12 (the region where the mask member 14 is not arranged (the region other than the region shown by the diagonal line in FIGS. 1C and 1D)).
  • a silver-plated film 16 is formed on the surface, and then the mask member 14 is removed (for example, the masking tape or resist mask is peeled off) as shown in FIGS. 1E and 2E.
  • the formation of the silver plating film 16 is preferably performed by electroplating.
  • the mask member 18 is arranged (for example, masking) on a portion other than a part of the other portion of the surface of the nickel plating film 12 and (the entire surface) of the silver plating film 16.
  • a portion of the other portion of the surface of the nickel plating film 12 (mask member 18 is placed) as shown in FIGS. 1G and 2G.
  • a tin-plated film 20 is formed in the non-existing areas (areas other than the areas shown by diagonal lines in FIGS. 1F and 1G), and then the mask member 18 is removed (for example, masking tape) as shown in FIGS. 1H and 2H. Or peel off the resist mask).
  • the tin plating film 20 is preferably formed by electroplating.
  • a plating material in which a silver plating film 16 and a tin plating film 20 (separated from the silver plating film 16) were formed on the surface of the nickel plating film 12 formed on substantially the entire surface of the base material 10 was produced. After that, using a furnace using a ceramics panel heater or the like, preheating is performed under the condition that the tin plating film 20 does not melt, and then, as shown in FIGS. 1J and 2J, the surface of the plating material (by an infrared lamp or the like).
  • the tin plating film 20 is melted and then cooled (reflow treatment) to form the tin plating film 20 into a reflow tin plating layer 22.
  • heating by infrared rays is radiation, and silver does not easily absorb infrared rays, and its absorption rate is, for example, about 0.01 at a wavelength of 1 ⁇ m, whereas tin easily absorbs infrared rays and its absorption rate. Is, for example, about 0.25 at a wavelength of 1 ⁇ m. Therefore, when the plating material on which the silver plating film 16 and the tin plating film 20 are formed on the surface of the nickel plating film 12 formed on substantially the entire surface of the base material 10 is heated by irradiating infrared rays with an infrared lamp or the like, silver plating is performed.
  • the film 16 is hardly heated by radiation, and the tin plating film 20 is selectively heated, so that the tin plating film 20 is melted and then cooled (reflow treatment), and the tin plating film 20 is reflowed to the tin plating layer 22.
  • reflow treatment a treatment for heating by infrared rays.
  • the base material 10 is a strip material, it is preferable to continuously plate by a reel-to-reel type continuous plating line.
  • the masking tape is used as the mask member 18, it is preferable that the masking tape is also continuously attached by the continuous tape attaching device in the continuous plating line.
  • the following embodiment of the plating material according to the present invention can be manufactured.
  • the nickel plating layer 12 is formed on substantially the entire surface of the base material 10 made of copper or a copper alloy, and the silver plating layer 16 is formed on a part of the surface of the nickel plating layer 12.
  • the reflow tin plating layer 22 is formed on a part of the other part of the surface of the nickel plating film 12 (away from the silver plating layer 16), and the contact resistance of the surface of the silver plating layer 16 is increased. It is 1 m ⁇ or less.
  • a strip material made of a Cu—Ni—Sn-based alloy (NB109-EH material manufactured by DOWA Metal Co., Ltd.) having a thickness of 0.2 mm and a width of 25 mm is prepared as a base material (material to be plated), and this strip material is used. It was installed in a reel-to-reel type continuous plating line so that the width direction is the vertical direction (continuous plating is applied).
  • the material to be plated and the SUS plate are put into an alkaline degreasing solution, the material to be plated is used as a cathode, the SUS plate is used as an anode, and electrolytic degreasing is performed at a voltage of 5 V for 30 seconds. After washing with water, pickling was performed in 3% sulfuric acid for 15 seconds.
  • a matte nickel plating solution consisting of an aqueous solution containing 540 g / L of nickel sulfamate tetrahydrate, 25 g / L of nickel chloride and 35 g / L of boric acid.
  • Electroplating was performed for 30 seconds at a liquid temperature of 50 ° C. and a current density of 9 A / dm 2 , using the material to be plated as a cathode and a nickel chip housed in a titanium anode case as an anode.
  • a matte nickel plating film was formed as a base plating film on almost the entire surface of both sides of the material to be plated.
  • the thickness of the matte nickel plating film at substantially the center in the width direction was measured by a fluorescent X-ray film thickness meter (SFT-110A manufactured by Hitachi High-Tech Science Corporation) and found to be 0.5 ⁇ m.
  • masking tape was attached to the portion of the base material (material to be plated) having a width of 13 mm from the lower end in the width direction and the portion having a width of 4 mm from the upper end in the width direction.
  • a silver strike plating solution consisting of an aqueous solution containing 3 g / L of silver potassium cyanide and 90 g / L of potassium cyanide
  • the base material on which the base plating film is formed is used as a cathode
  • stainless steel (SUS) is used.
  • silver plating consisting of an aqueous solution containing 175 g / L of silver potassium cyanide (KAg (CN) 2 ), 95 g / L of potassium cyanide (KCN) and 102 mg / L of potassium selenocyanate (KSeCN).
  • the base material on which the silver strike plating film is formed is used as the cathode, and the silver particles housed in the titanium anode case are used as the anode, and electroplating (silver) at a liquid temperature of 18 ° C. and a current density of 8 A / dm 2 for 21 seconds.
  • Plating was performed to form a silver plating film on the substrate (on the silver strike plating film), which was then washed with water to thoroughly wash away the silver plating solution.
  • the thickness of the silver-plated film at substantially the center in the width direction was measured by a fluorescent X-ray film thickness meter (SFT-110A manufactured by Hitachi High-Tech Science Corporation) and found to be 1.0 ⁇ m.
  • the portion 15 mm wide from the upper end in the width direction of the base material covering the entire surface of the silver plating film and a part of the base plating film). A masking tape was attached to the strip).
  • tin alkanolsulfonate (as metal tin salt) (Metas SM-2 manufactured by Yuken Kogyo Co., Ltd.) and alkanolsulfonic acid (metas manufactured by Yuken Kogyo Co., Ltd.) AM)
  • a tin plating solution containing 75 mL / L the base material on which the silver plating film was formed was used as the cathode, and the tin balls housed in the titanium anode case were used as the anode, and the solution temperature was 25 ° C. and the current density was 12 A.
  • Electroplating (tin plating) was performed for 14 seconds at / dm 2 , and the area on the base material where the masking tape was not attached (the exposed surface of the base plating film on the base material (width from the lower end in the width direction of the material to be plated). After forming a tin-plated film having a thickness of 1 ⁇ m in a 10 mm region)), the masking tape was peeled off.
  • the base material on which the tin-plated film was formed was placed in a furnace using a ceramic panel heater, preheated in this furnace (the tin-plated film was not melted by this preheating), and then a flat plate surface was formed.
  • the reflow treatment was performed by facing a radial infrared lamp (Ps110VP manufactured by Advance Riko Co., Ltd., single layer 200V, 2kW) and heating at an output of 67% for 15 seconds. It was confirmed that the tin plating layer was melted and then solidified by this reflow treatment to form the reflow tin plating layer.
  • the contact resistance on the surface of the silver plating layer was measured before and after the reflow treatment with an electric contact simulator (CRS-1 manufactured by Yamasaki Seiki Laboratory Co., Ltd.) under a load of 100 gf. It was 0.72 m ⁇ before and 0.64 m ⁇ after the reflow treatment, and there was no increase in contact resistance. Moreover, when the appearance of the silver-plated layer was visually observed, no discoloration was confirmed before and after the reflow treatment.
  • an electric contact simulator CRS-1 manufactured by Yamasaki Seiki Laboratory Co., Ltd.
  • Base material 12
  • Mask member 16
  • Silver plating film 18
  • Mask member 20
  • Tin plating film 22

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Composite Materials (AREA)
  • Electroplating Methods And Accessories (AREA)

Abstract

Provided are: a plated material in which a silver plating film is formed on a part of the surface thereof and a tin plating film is formed on a different part of the surface thereof, and is prevented from the increase in the contact resistance of the silver plating film and the discoloration of the surface after a reflow treatment of the plated material, and is inexpensive; and a method for manufacturing the plated material. A nickel plating film 12 is formed on the surface of a base material 10 made from copper or a copper alloy, a silver plating film 16 is then formed on a part of the surface of the nickel plating film 12, and a tin plating film 20 is then formed on a part of an area excluding the above-mentioned part in the surface of the nickel plating film 12, thereby manufacturing a plated material in which the silver plating film 16 and the tin plating film 20 are formed on the surface of the nickel plating film 12 formed on the base material 10. Subsequently, the tin plating film 20 is subjected to a reflow treatment comprising heating the surface of the plated material by the irradiation with infrared ray, thereby converting the tin plating film 20 to a reflow tin plating layer 22.

Description

めっき材およびその製造方法Plating material and its manufacturing method
　本発明は、めっき材およびその製造方法に関し、特に、車載用や民生用の電気配線に使用されるコネクタ、スイッチ、リレーなどの接点や端子部品の材料として使用されるめっき材およびその製造方法に関する。 The present invention relates to a plating material and a method for manufacturing the same, and more particularly to a plating material used as a material for contacts and terminal parts such as connectors, switches, and relays used for in-vehicle and consumer electrical wiring, and a method for manufacturing the same. ..
　従来、コネクタやスイッチなどの接点や端子部品などの材料として、銅または銅合金やステンレス鋼などの比較的安価で耐食性や機械的特性などに優れた基材に、電気特性や半田付け性などの必要な特性に応じて、錫、銀、金などのめっきを施しためっき材が使用されている。これらのめっきと基材との間の密着性を向上させるために、これらのめっきと基材との間にニッケルからなる下地層を形成しためっき材も使用されている。 Conventionally, as a material for contacts and terminal parts such as connectors and switches, a relatively inexpensive base material such as copper or copper alloy or stainless steel, which has excellent corrosion resistance and mechanical properties, has electrical properties and solderability. Plating materials plated with tin, silver, gold, etc. are used, depending on the required properties. In order to improve the adhesion between these platings and the base material, a plating material in which a base layer made of nickel is formed between these platings and the base material is also used.
　銅または銅合金やステンレス鋼などの基材に錫めっきを施した錫めっき材は、安価であるが、高温環境下における耐食性に劣っている。また、これらの基材に金めっきを施した金めっき材は、耐食性に優れ、信頼性が高いが、コストが高くなる。一方、これらの基材に銀めっきを施した銀めっき材は、金めっき材と比べて安価であり、錫めっき材と比べて耐食性に優れている。 A tin-plated material obtained by tin-plating a base material such as copper or a copper alloy or stainless steel is inexpensive, but inferior in corrosion resistance in a high temperature environment. Further, the gold-plated material obtained by subjecting these base materials to gold plating has excellent corrosion resistance and high reliability, but the cost is high. On the other hand, the silver-plated material obtained by silver-plating these base materials is cheaper than the gold-plated material and has excellent corrosion resistance as compared with the tin-plated material.
　そのため、コネクタなどの端子部品の材料として、雄端子と雌端子が嵌合する部分（嵌合部）に金や銀めっきが施され、電線などを加締める部分（加締め部）に安価で変形し易い光沢錫めっきや無光沢錫めっきが施されためっき材が使用される場合がある。 Therefore, as a material for terminal parts such as connectors, the part where the male terminal and the female terminal are fitted (fitting part) is plated with gold or silver, and the part where the electric wire is crimped (the crimping part) is inexpensively deformed. A plating material with glossy tin plating or matte tin plating, which is easy to use, may be used.
　また、一般に、錫めっきは、電気めっきによって行われており、錫めっき皮膜の内部応力を緩和してウイスカの発生を抑制するために、電気めっきの後にリフロー処理（加熱により錫めっきを溶融した後に凝固させる処理）が行われている。このように錫めっき後にリフロー処理を行うと、錫の一部が素材や下地成分に拡散して化合物層を形成し、この化合物層上に錫または錫合金層が形成される。 In addition, tin plating is generally performed by electroplating, and in order to alleviate the internal stress of the tin plating film and suppress the generation of whiskers, reflow treatment (after melting the tin plating by heating) is performed after electroplating. Processing to solidify) is being performed. When the reflow treatment is performed after tin plating in this way, a part of tin diffuses into the material and the base component to form a compound layer, and a tin or tin alloy layer is formed on the compound layer.
　特に、アルミニウムまたはアルミニウム合金からなる電線などを加締める部分に錫めっきが施されためっき材では、抵抗値が高くなるので、抵抗値の上昇を抑制するために錫めっきを施した後でリフロー処理を施す必要がある。 In particular, a plating material in which the part where an electric wire made of aluminum or an aluminum alloy is crimped is tin-plated has a high resistance value. Therefore, in order to suppress an increase in the resistance value, a reflow treatment is performed after tin plating. Need to be applied.
　このようなめっき材として、銅または銅合金からなる板状金属部材の一方の面に電解めっきによりニッケルの下地めっき層を形成し、この下地めっき層上に電解めっきにより銀めっき層を形成し、板状金属部材の他方の面に下地なしで直接電解めっきにより錫めっき層を形成した後、酸素濃度が２００ｐｐｍ以下の低酸素濃度雰囲気中で４００～８００℃に加熱するリフロー処理を行って錫めっき層を溶融させることにより板状金属部材と錫めっき層の間に錫－銅の金属間化合物を形成することが知られている（例えば、特許文献１参照）。 As such a plating material, a nickel base plating layer is formed by electroplating on one surface of a plate-shaped metal member made of copper or a copper alloy, and a silver plating layer is formed on the base plating layer by electroplating. A tin-plated layer is formed on the other surface of the plate-shaped metal member by direct electroplating without a base, and then reflowed by heating to 400 to 800 ° C. in a low oxygen concentration atmosphere with an oxygen concentration of 200 ppm or less to perform tin plating. It is known that a tin-copper metal-to-metal compound is formed between a plate-shaped metal member and a tin-plated layer by melting the layer (see, for example, Patent Document 1).
　また、少なくとも一部にリフロー錫めっき層が形成され、このリフロー錫めっき層との界面に反応層が形成された金属基材から、リフロー錫めっき層と反応層の少なくとも一部を完全に剥離させ、リフロー錫めっき層と反応層を完全に剥離させた領域の少なくとも一部にニッケルめっき処理を施してニッケルめっき層を形成し、このニッケルめっき層の少なくとも一部に錫めっき処理を施すことが知られている（例えば、特許文献２参照）。 Further, at least a part of the reflow tin plating layer and the reaction layer is completely peeled off from the metal base material in which the reflow tin plating layer is formed at least partially and the reaction layer is formed at the interface with the reflow tin plating layer. It is known that at least a part of the region where the reflow tin plating layer and the reaction layer are completely peeled off is subjected to a nickel plating treatment to form a nickel plating layer, and at least a part of this nickel plating layer is subjected to a tin plating treatment. (See, for example, Patent Document 2).
特開２００２－１３４３６１号公報（段落番号００３３）JP-A-2002-134361 (paragraph number 0033) 国際公開ＷＯ２０１５／０９２９７９号公報（段落番号００１１）International Publication WO2015 / 092979 (paragraph number 0011)
　コネクタなどの端子部品の材料として使用するめっき材が、嵌合部に（耐酸化性に優れた）金めっきが施され、加締め部に錫めっきが施された後にリフロー処理を施されためっき材である場合には、リフロー処理による加熱後も接触抵抗がほとんど上昇しない。しかし、コネクタなどの端子部品の材料として使用するめっき材が、嵌合部に（金めっきと比べて安価な）銀めっきが施され、加締め部に錫めっきが施された後にリフロー処理を施されためっき材である場合には、リフロー処理による加熱後に銀めっき皮膜の接触抵抗が上昇したり、銀めっき皮膜の表面が変色するという問題がある。 The plating material used as a material for terminal parts such as connectors is plated with gold plating (excellent oxidation resistance) at the fitting part, tin plating at the crimping part, and then reflow processing. In the case of a material, the contact resistance hardly increases even after heating by the reflow treatment. However, the plating material used as the material for terminal parts such as connectors is silver-plated (cheaper than gold plating) on the fitting part, tin-plated on the crimped part, and then reflowed. In the case of the plated material, there is a problem that the contact resistance of the silver plating film increases after heating by the reflow treatment and the surface of the silver plating film is discolored.
　特許文献１の方法では、低酸素濃度雰囲気中で加熱するための設備が必要になり、製造コストが高くなる。また、低酸素濃度雰囲気中でリフロー処理を行っても、銀めっき層と錫めっき層が共存する状態で高温で加熱するため、銀めっき層の接触抵抗が上昇したり、銀めっき層の表面が変色するおそれがある。 The method of Patent Document 1 requires equipment for heating in a low oxygen concentration atmosphere, which increases the manufacturing cost. In addition, even if the reflow treatment is performed in a low oxygen concentration atmosphere, the contact resistance of the silver plating layer increases and the surface of the silver plating layer becomes high because the silver plating layer and the tin plating layer coexist and are heated at a high temperature. There is a risk of discoloration.
　特許文献２の方法では、リフロー錫めっき層と反応層の少なくとも一部を完全に剥離させる工程が必要になり、製造コストが高くなる。また、薬液で溶解させて剥離する際に必要以上にリフロー錫めっき層や反応層が剥離されるおそれがある。 The method of Patent Document 2 requires a step of completely peeling off at least a part of the reflow tin plating layer and the reaction layer, which increases the manufacturing cost. In addition, the reflow tin plating layer and the reaction layer may be peeled off more than necessary when they are dissolved in a chemical solution and peeled off.
　したがって、本発明は、このような従来の問題点に鑑み、表面の一部に銀めっき皮膜が形成されるとともに他の一部に錫めっき皮膜が形成されためっき材をリフロー処理した後に銀めっき皮膜の接触抵抗の上昇や表面の変色を防止することができる、安価なめっき材およびその製造方法を提供することを目的とする。 Therefore, in view of such conventional problems, the present invention reflows a plating material having a silver-plated film formed on a part of the surface and a tin-plated film formed on the other part, and then silver-plated. It is an object of the present invention to provide an inexpensive plating material and a method for producing the same, which can prevent an increase in contact resistance of the film and discoloration of the surface.
　本発明者らは、上記課題を解決するために鋭意研究した結果、銅または銅合金からなる基材の表面にニッケルめっき皮膜を形成し、このニッケルめっき皮膜の表面の一部に銀めっき皮膜を形成するとともに、ニッケルめっき皮膜の表面の他の部分の一部に錫めっき皮膜を形成することにより、基材上のニッケルめっき皮膜の表面に銀めっき皮膜と錫めっき皮膜が形成されためっき材を作製した後、このめっき材の表面に赤外線を照射して加熱することにより、錫めっき皮膜をリフロー処理して、錫めっき皮膜をリフロー錫めっき層にすれば、錫めっき皮膜をリフロー処理した後に銀めっき皮膜の接触抵抗の上昇や表面の変色を防止することができる、めっき材を低コストで製造することができることを見出し、本発明を完成するに至った。 As a result of diligent research to solve the above problems, the present inventors formed a nickel-plated film on the surface of a base material made of copper or a copper alloy, and formed a silver-plated film on a part of the surface of the nickel-plated film. A plating material in which a silver plating film and a tin plating film are formed on the surface of the nickel plating film on the base material is formed by forming the tin plating film on a part of the other part of the surface of the nickel plating film. After the production, the surface of this plating material is irradiated with infrared rays and heated to reflow the tin plating film, and if the tin plating film is made into a reflow tin plating layer, the tin plating film is reflowed and then silver. We have found that a plating material can be manufactured at low cost, which can prevent an increase in the contact resistance of the plating film and discoloration of the surface, and have completed the present invention.
　すなわち、本発明によるめっき材の製造方法は、銅または銅合金からなる基材の表面にニッケルめっき皮膜を形成し、このニッケルめっき皮膜の表面の一部に銀めっき皮膜を形成するとともに、ニッケルめっき皮膜の表面の他の部分の一部に錫めっき皮膜を形成することにより、基材上のニッケルめっき皮膜の表面に銀めっき皮膜と錫めっき皮膜が形成されためっき材を作製した後、このめっき材の表面に赤外線を照射して加熱することにより、錫めっき皮膜をリフロー処理して、錫めっき皮膜をリフロー錫めっき層にすることを特徴とする。 That is, in the method for producing a plating material according to the present invention, a nickel plating film is formed on the surface of a base material made of copper or a copper alloy, a silver plating film is formed on a part of the surface of the nickel plating film, and nickel plating is performed. By forming a tin-plated film on a part of the other part of the surface of the film, a plating material in which a silver-plated film and a tin-plated film are formed on the surface of the nickel-plated film on the base material is produced, and then this plating is performed. By irradiating the surface of the material with infrared rays and heating it, the tin-plated film is reflowed to form a reflowed tin-plated layer.
　このめっき材の製造方法において、赤外線の照射の前に、ニッケルめっき皮膜の表面に銀めっき皮膜と錫めっき皮膜が形成されためっき材を、錫めっき皮膜が溶融しないように予備加熱するのが好ましい。また、赤外線の照射が、赤外線ランプにより行われるのが好ましい。さらに、ニッケルめっき皮膜の表面の一部と、ニッケルめっき皮膜の表面の他の部分の一部が離間しているのが好ましい。 In this method for producing a plating material, it is preferable to preheat a plating material in which a silver plating film and a tin plating film are formed on the surface of the nickel plating film before irradiation with infrared rays so that the tin plating film does not melt. .. Further, it is preferable that infrared irradiation is performed by an infrared lamp. Further, it is preferable that a part of the surface of the nickel plating film and a part of the other part of the surface of the nickel plating film are separated from each other.
　また、上記のめっき材の製造方法において、銀めっき皮膜を形成した後に錫めっき皮膜を形成するのが好ましい。この場合、ニッケルめっき皮膜を形成した後、銀めっき皮膜を形成する前に、ニッケルめっき皮膜の表面の一部以外の部分をマスク部材によって覆うのが好ましい。また、銀めっき皮膜を形成した後、錫めっき皮膜を形成する前に、ニッケルめっき皮膜の他の表面の一部以外の部分と銀めっき皮膜の表面をマスク部材によって覆うのが好ましい。 Further, in the above method for producing a plating material, it is preferable to form a tin plating film after forming a silver plating film. In this case, it is preferable to cover a portion other than a part of the surface of the nickel plating film with a mask member after forming the nickel plating film and before forming the silver plating film. Further, after the silver plating film is formed and before the tin plating film is formed, it is preferable to cover a portion other than a part of the other surface of the nickel plating film and the surface of the silver plating film with a mask member.
　また、本発明によるめっき材は、銅または銅合金からなる基材の表面にニッケルめっき層が形成され、このニッケルめっき層の表面の一部に銀めっき層が形成されているとともに、ニッケルめっき皮膜の表面の他の部分の一部にリフロー錫めっき層が形成され、銀めっき層の表面の接触抵抗が１ｍΩ以下であることを特徴とする。 Further, in the plating material according to the present invention, a nickel plating layer is formed on the surface of a base material made of copper or a copper alloy, a silver plating layer is formed on a part of the surface of the nickel plating layer, and a nickel plating film is formed. A reflow tin plating layer is formed on a part of the other portion of the surface of the silver plating layer, and the contact resistance of the surface of the silver plating layer is 1 mΩ or less.
　このめっき材において、ニッケルめっき層の表面に形成されている銀めっき層と錫めっき層が離間しているのが好ましい。 In this plating material, it is preferable that the silver plating layer and the tin plating layer formed on the surface of the nickel plating layer are separated from each other.
　本発明によれば、表面の一部に銀めっき皮膜が形成されるとともに他の一部に錫めっき皮膜が形成されためっき材をリフロー処理した後に銀めっき皮膜の接触抵抗の上昇や表面の変色を低コストで防止することができる、安価なめっき材を製造することができる。 According to the present invention, after reflowing a plating material in which a silver plating film is formed on a part of the surface and a tin plating film is formed on another part, the contact resistance of the silver plating film is increased and the surface is discolored. It is possible to manufacture an inexpensive plating material that can prevent the above-mentioned problems at low cost.
本発明によるめっき材の製造方法の実施の形態において基材を用意する工程を説明する平面図である。It is a top view explaining the process of preparing a base material in embodiment of the method of manufacturing a plating material by this invention. 本発明によるめっき材の製造方法の実施の形態においてニッケルめっき皮膜を形成する工程を説明する平面図である。It is a top view explaining the process of forming a nickel plating film in embodiment of the method of manufacturing a plating material by this invention. 本発明によるめっき材の製造方法の実施の形態においてニッケルめっき皮膜の一部にマスキングテープを貼る工程を説明する平面図である。It is a top view explaining the process of attaching a masking tape to a part of a nickel plating film in embodiment of the method of manufacturing a plating material by this invention. 本発明によるめっき材の製造方法の実施の形態においてニッケルめっき皮膜のマスキングテープが貼られていない部分に銀めっき皮膜を形成する工程を説明する平面図である。It is a top view explaining the process of forming a silver plating film in the part where the masking tape of a nickel plating film is not attached in embodiment of the method of manufacturing a plating material by this invention. 本発明によるめっき材の製造方法の実施の形態において銀めっき皮膜を形成した後にマスキングテープを剥離する工程を説明する平面図である。It is a top view explaining the step of peeling off a masking tape after forming a silver plating film in embodiment of the method of manufacturing a plating material by this invention. 本発明によるめっき材の製造方法の実施の形態においてマスキングテープを剥離した後に銀めっき皮膜の全面とニッケルめっき皮膜の一部にマスキングテープを貼る工程を説明する平面図である。It is a top view explaining the process of attaching the masking tape to the whole surface of the silver plating film and a part of the nickel plating film after peeling off the masking tape in the embodiment of the method for manufacturing a plating material according to the present invention. 本発明によるめっき材の製造方法の実施の形態においてニッケルめっき皮膜のマスキングテープが貼られていない部分に錫めっき皮膜を形成する工程を説明する平面図である。It is a top view explaining the process of forming a tin plating film in the part where the masking tape of a nickel plating film is not attached in embodiment of the method of manufacturing a plating material by this invention. 本発明によるめっき材の製造方法の実施の形態において錫めっき皮膜を形成した後にマスキングテープを剥離する工程を説明する平面図である。It is a top view explaining the step of peeling off a masking tape after forming a tin plating film in embodiment of the method of manufacturing a plating material by this invention. 本発明によるめっき材の製造方法の実施の形態においてマスキングテープを剥離した後に錫めっき皮膜のリフロー処理を行う工程を説明する平面図である。It is a top view explaining the step of performing a reflow treatment of a tin plating film after peeling off a masking tape in embodiment of the method of manufacturing a plating material by this invention. 図１ＡのＩＩＡ－ＩＩＡ線断面図である。FIG. 1A is a sectional view taken along line IIA-IIA of FIG. 1A. 図１ＢのＩＩＢ－ＩＩＢ線断面図である。FIG. 1B is a sectional view taken along line IIB-IIB of FIG. 1B. 図１ＣのＩＩＣ－ＩＩＣ線断面図である。FIG. 1C is a sectional view taken along line IIC-IIC of FIG. 1C. 図１ＤのＩＩＤ－ＩＩＤ線断面図である。FIG. 3 is a cross-sectional view taken along line IID-IID of FIG. 1D. 図１ＥのＩＩＥ－ＩＩＥ線断面図である。It is a cross-sectional view taken along the line IIE-IIE of FIG. 1E. 図１ＦのＩＩＦ－ＩＩＦ線断面図である。FIG. 2 is a sectional view taken along line IIF-IIF of FIG. 1F. 図１ＧのＩＩＧ－ＩＩＧ線断面図である。FIG. 5 is a cross-sectional view taken along the line IIG-IIG of FIG. 図１ＨのＩＩＨ－ＩＩＧ線断面図である。FIG. 2 is a sectional view taken along line IIH-IIG of FIG. 1H. 図１ＪのＩＩＪ－ＩＩＪ線断面図である。FIG. 2 is a sectional view taken along line IIJ-IIJ of FIG. 1J.
　以下、添付図面を参照して、本発明によるめっき材の製造方法の実施の形態について詳細に説明する。 Hereinafter, embodiments of the method for producing a plating material according to the present invention will be described in detail with reference to the attached drawings.
　本発明によるめっき材の製造方法の実施の形態では、図１Ａおよび図２Ａに示すように、銅または銅合金からなる基材１０を用意する。この基材１０として、無酸素銅やタフピッチ銅などの純銅系の基材や、黄銅、りん青銅、Ｃｕ－Ｎｉ－Ｓｉ系合金、Ｃｕ－Ｆｅ－Ｐ系合金、Ｃｕ－Ｎｉ－Ｓｎ－Ｐ系合金などの銅合金からなる基材を使用することができる。また、基材１０の形状は、短冊状の個片でもよいが、生産性の面から（リール・トゥ・リール方式の連続めっきラインによってめっき材を製造することができる）条材であるのが好ましい。 In the embodiment of the method for producing a plating material according to the present invention, as shown in FIGS. 1A and 2A, a base material 10 made of copper or a copper alloy is prepared. The base material 10 includes pure copper-based base materials such as oxygen-free copper and tough pitch copper, brass, phosphorous bronze, Cu-Ni-Si-based alloys, Cu-Fe-P-based alloys, and Cu-Ni-Sn-P-based base materials. A base material made of a copper alloy such as an alloy can be used. Further, the shape of the base material 10 may be a strip-shaped individual piece, but from the viewpoint of productivity (a plating material can be manufactured by a reel-to-reel type continuous plating line), a strip material is used. preferable.
　次に、図１Ｂおよび図２Ｂに示すように、基材１０の表面（圧延面）の略全面に下地めっき皮膜としてニッケルめっき皮膜１２を形成する。このニッケルめっき皮膜の形成は、電気めっきまたは無電解めっきのいずれでもよいが、生産性やコスト面から電気めっきによって行うのが好ましい。 Next, as shown in FIGS. 1B and 2B, a nickel plating film 12 is formed as a base plating film on substantially the entire surface (rolled surface) of the base material 10. The nickel plating film may be formed by either electroplating or electroless plating, but it is preferably performed by electroplating from the viewpoint of productivity and cost.
　次に、図１Ｃおよび図２Ｃに示すように、ニッケルめっき皮膜１２の表面の一部以外の部分にマスク部材１４を配置（例えば、マスキングテープを貼り付けるか、レジストマスクを形成）してその部分を覆った後、図１Ｄおよび図２Ｄに示すように、ニッケルめっき皮膜１２の表面の一部（マスク部材１４を配置していない領域（図１Ｃおよび図１Ｄにおいて斜線で示す領域以外の領域））に銀めっき皮膜１６を形成し、その後、図１Ｅおよび図２Ｅに示すように、マスク部材１４を除去（例えば、マスキングテープまたはレジストマスクを剥離）する。この銀めっき皮膜１６の形成は、電気めっきによって行うのが好ましい。 Next, as shown in FIGS. 1C and 2C, a mask member 14 is arranged (for example, a masking tape is attached or a resist mask is formed) on a portion other than a part of the surface of the nickel plating film 12, and that portion is formed. As shown in FIGS. 1D and 2D, a part of the surface of the nickel plating film 12 (the region where the mask member 14 is not arranged (the region other than the region shown by the diagonal line in FIGS. 1C and 1D)). A silver-plated film 16 is formed on the surface, and then the mask member 14 is removed (for example, the masking tape or resist mask is peeled off) as shown in FIGS. 1E and 2E. The formation of the silver plating film 16 is preferably performed by electroplating.
　次に、図１Ｆおよび図２Ｆに示すように、ニッケルめっき皮膜１２の表面の他の部分の一部以外の部分と銀めっき皮膜１６の表面（の全面）にマスク部材１８を配置（例えば、マスキングテープを貼り付けるか、レジストマスクを形成）してその部分を覆った後、図１Ｇおよび図２Ｇに示すように、ニッケルめっき皮膜１２の表面の他の部分の一部（マスク部材１８を配置していない領域（図１Ｆおよび図１Ｇにおいて斜線で示す領域以外の領域））に錫めっき皮膜２０を形成し、その後、図１Ｈおよび図２Ｈに示すように、マスク部材１８を除去（例えば、マスキングテープまたはレジストマスクを剥離）する。この錫めっき皮膜２０の形成は、電気めっきによって行うのが好ましい。 Next, as shown in FIGS. 1F and 2F, the mask member 18 is arranged (for example, masking) on a portion other than a part of the other portion of the surface of the nickel plating film 12 and (the entire surface) of the silver plating film 16. After affixing tape (or forming a resist mask) to cover that portion, a portion of the other portion of the surface of the nickel plating film 12 (mask member 18 is placed) as shown in FIGS. 1G and 2G. A tin-plated film 20 is formed in the non-existing areas (areas other than the areas shown by diagonal lines in FIGS. 1F and 1G), and then the mask member 18 is removed (for example, masking tape) as shown in FIGS. 1H and 2H. Or peel off the resist mask). The tin plating film 20 is preferably formed by electroplating.
　このようにして基材１０の略全面に形成されたニッケルめっき皮膜１２の表面に銀めっき皮膜１６と（この銀めっき皮膜１６から離間して）錫めっき皮膜２０が形成されためっき材を作製した後、セラミックスパネルヒーターなどを用いた炉を使用して、錫めっき皮膜２０が溶融しない条件で予備加熱した後、図１Ｊおよび図２Ｊに示すように、そのめっき材の表面に（赤外線ランプなどにより）大気中で赤外線を照射して加熱することにより、錫めっき皮膜２０を溶融した後に冷却（リフロー処理）して、錫めっき皮膜２０をリフロー錫めっき層２２にする。 In this way, a plating material in which a silver plating film 16 and a tin plating film 20 (separated from the silver plating film 16) were formed on the surface of the nickel plating film 12 formed on substantially the entire surface of the base material 10 was produced. After that, using a furnace using a ceramics panel heater or the like, preheating is performed under the condition that the tin plating film 20 does not melt, and then, as shown in FIGS. 1J and 2J, the surface of the plating material (by an infrared lamp or the like). ) By irradiating infrared rays in the atmosphere and heating, the tin plating film 20 is melted and then cooled (reflow treatment) to form the tin plating film 20 into a reflow tin plating layer 22.
　なお、赤外線による加熱は輻射であり、銀は赤外線を吸収し難く、その吸収率は、例えば、波長１μｍで０．０１程度であるのに対して、錫は赤外線を吸収し易く、その吸収率は、例えば、波長１μｍで０．２５程度である。そのため、基材１０の略全面に形成されたニッケルめっき皮膜１２の表面に銀めっき皮膜１６と錫めっき皮膜２０が形成されためっき材に、赤外線ランプなどにより赤外線を照射して加熱すると、銀めっき皮膜１６は輻射によりほとんど加熱されず、錫めっき皮膜２０が選択的に加熱されることにより、錫めっき皮膜２０が溶融した後に冷却（リフロー処理）されて、錫めっき皮膜２０がリフロー錫めっき層２２になると考えられる。このようにしてリフロー錫めっき層２２を形成すると、加熱による銀めっき皮膜の昇温が抑制されるため、銀めっき皮膜の変色が抑制され、接触抵抗の上昇も抑制されると考えられる。また、赤外線による加熱の前に、錫めっき皮膜が溶融しない程度に予備加熱しておけば、赤外線による加熱の時間を短縮することができる。 It should be noted that heating by infrared rays is radiation, and silver does not easily absorb infrared rays, and its absorption rate is, for example, about 0.01 at a wavelength of 1 μm, whereas tin easily absorbs infrared rays and its absorption rate. Is, for example, about 0.25 at a wavelength of 1 μm. Therefore, when the plating material on which the silver plating film 16 and the tin plating film 20 are formed on the surface of the nickel plating film 12 formed on substantially the entire surface of the base material 10 is heated by irradiating infrared rays with an infrared lamp or the like, silver plating is performed. The film 16 is hardly heated by radiation, and the tin plating film 20 is selectively heated, so that the tin plating film 20 is melted and then cooled (reflow treatment), and the tin plating film 20 is reflowed to the tin plating layer 22. Is thought to be. When the reflow tin plating layer 22 is formed in this way, it is considered that the temperature rise of the silver plating film due to heating is suppressed, so that the discoloration of the silver plating film is suppressed and the increase in contact resistance is also suppressed. Further, if the tin plating film is preheated to the extent that it does not melt before heating by infrared rays, the time for heating by infrared rays can be shortened.
　基材１０が条材である場合には、リール・トゥ・リール方式の連続めっきラインによって、連続的にめっきするのが好ましい。また、マスク部材１８としてマスキングテープを使用する場合には、連続めっきラインにおいて、マスキングテープも連続テープ貼り装置によって連続的に貼り付けるのが好ましい。 When the base material 10 is a strip material, it is preferable to continuously plate by a reel-to-reel type continuous plating line. When the masking tape is used as the mask member 18, it is preferable that the masking tape is also continuously attached by the continuous tape attaching device in the continuous plating line.
　上述しためっき材の製造方法の実施の形態により、以下のような本発明によるめっき材の実施の形態を製造することができる。 According to the embodiment of the plating material manufacturing method described above, the following embodiment of the plating material according to the present invention can be manufactured.
　本発明によるめっき材の実施の形態は、銅または銅合金からなる基材１０の表面の略全面にニッケルめっき層１２が形成され、このニッケルめっき層１２の表面の一部に銀めっき層１６が形成されているとともに、（この銀めっき層１６から離間して）ニッケルめっき皮膜１２の表面の他の部分の一部にリフロー錫めっき層２２が形成され、銀めっき層１６の表面の接触抵抗が１ｍΩ以下である。 In the embodiment of the plating material according to the present invention, the nickel plating layer 12 is formed on substantially the entire surface of the base material 10 made of copper or a copper alloy, and the silver plating layer 16 is formed on a part of the surface of the nickel plating layer 12. Along with the formation, the reflow tin plating layer 22 is formed on a part of the other part of the surface of the nickel plating film 12 (away from the silver plating layer 16), and the contact resistance of the surface of the silver plating layer 16 is increased. It is 1 mΩ or less.
　以下、本発明によるめっき材およびその製造方法の実施例について詳細に説明する。 Hereinafter, examples of the plating material according to the present invention and the method for producing the same will be described in detail.
［実施例］
　まず、基材（被めっき材）として厚さ０．２ｍｍで幅２５ｍｍのＣｕ－Ｎｉ－Ｓｎ系合金（ＤＯＷＡメタル株式会社製のＮＢ１０９－ＥＨ材）からなる条材を用意し、この条材をその幅方向が鉛直方向になるように（連続的にめっきを施す）リール・トゥ・リール方式の連続めっきラインに設置した。 [Example]
First, a strip material made of a Cu—Ni—Sn-based alloy (NB109-EH material manufactured by DOWA Metal Co., Ltd.) having a thickness of 0.2 mm and a width of 25 mm is prepared as a base material (material to be plated), and this strip material is used. It was installed in a reel-to-reel type continuous plating line so that the width direction is the vertical direction (continuous plating is applied).
　この連続めっきラインにおいて、被めっき材の前処理として、被めっき材とＳＵＳ板をアルカリ脱脂液に入れ、被めっき材を陰極とし、ＳＵＳ板を陽極として、電圧５Ｖで３０秒間電解脱脂を行い、水洗した後、３％硫酸中で１５秒間酸洗を行った。 In this continuous plating line, as a pretreatment of the material to be plated, the material to be plated and the SUS plate are put into an alkaline degreasing solution, the material to be plated is used as a cathode, the SUS plate is used as an anode, and electrolytic degreasing is performed at a voltage of 5 V for 30 seconds. After washing with water, pickling was performed in 3% sulfuric acid for 15 seconds.
　次に、連続めっきラインにおいて、５４０ｇ／Ｌのスルファミン酸ニッケル四水和物と２５ｇ／Ｌの塩化ニッケルと３５ｇ／Ｌのホウ酸を含む水溶液からなる無光沢ニッケルめっき液中において、前処理を行った被めっき材を陰極とし、チタン製のアノードケースに収容されたニッケルのチップを陽極として、液温５０℃において電流密度９Ａ／ｄｍ２で３０秒間電気めっき（無光沢ニッケルめっき）を行って、被めっき材の両面の略全面に下地めっき皮膜として無光沢ニッケルめっき皮膜を形成した。この無光沢ニッケルめっき皮膜の幅方向略中央部の厚さを蛍光Ｘ線膜厚計（株式会社日立ハイテクサイエンス製のＳＦＴ－１１０Ａ）により測定したところ、０．５μｍであった。 Next, in a continuous plating line, pretreatment is performed in a matte nickel plating solution consisting of an aqueous solution containing 540 g / L of nickel sulfamate tetrahydrate, 25 g / L of nickel chloride and 35 g / L of boric acid. Electroplating (matte nickel plating) was performed for 30 seconds at a liquid temperature of 50 ° C. and a current density of 9 A / dm 2 , using the material to be plated as a cathode and a nickel chip housed in a titanium anode case as an anode. A matte nickel plating film was formed as a base plating film on almost the entire surface of both sides of the material to be plated. The thickness of the matte nickel plating film at substantially the center in the width direction was measured by a fluorescent X-ray film thickness meter (SFT-110A manufactured by Hitachi High-Tech Science Corporation) and found to be 0.5 μm.
　次に、連続めっきラインにおいて、基材（被めっき材）の両面の幅方向下端部から幅１３ｍｍの部分と幅方向上端部から幅４ｍｍの部分にマスキングテープを貼り付けた。 Next, in the continuous plating line, masking tape was attached to the portion of the base material (material to be plated) having a width of 13 mm from the lower end in the width direction and the portion having a width of 4 mm from the upper end in the width direction.
　次に、連続めっきラインにおいて、３ｇ／Ｌのシアン化銀カリウムと９０ｇ／Ｌのシアン化カリウムを含む水溶液からなる銀ストライクめっき液中において、下地めっき皮膜を形成した基材を陰極とし、ステンレス（ＳＵＳ）板を陽極として、室温（２５℃）、電流密度２Ａ／ｄｍ２で１０秒間電気めっきを行うことにより、下地めっき皮膜を形成した基材上のマスキングテープが貼られていない領域（帯状の露出面）に銀ストライクめっき皮膜を形成した後、水洗して銀ストライクめっき液を十分に洗い流した。 Next, in a continuous plating line, in a silver strike plating solution consisting of an aqueous solution containing 3 g / L of silver potassium cyanide and 90 g / L of potassium cyanide, the base material on which the base plating film is formed is used as a cathode, and stainless steel (SUS) is used. By electroplating for 10 seconds at room temperature (25 ° C.) and current density of 2 A / dm 2 using the plate as the anode, the area (band-shaped exposed surface) on the base material on which the base plating film is formed and where the masking tape is not affixed. ) Was formed with a silver strike plating film, and then washed with water to thoroughly wash away the silver strike plating solution.
　次に、連続めっきラインにおいて、１７５ｇ／Ｌのシアン化銀カリウム（ＫＡｇ（ＣＮ）２）と９５ｇ／Ｌのシアン化カリウム（ＫＣＮ）と１０２ｍｇ／Ｌのセレノシアン酸カリウム（ＫＳｅＣＮ）を含む水溶液からなる銀めっき液中において、銀ストライクめっき皮膜を形成した基材を陰極とし、チタン製のアノードケースに収容された銀粒子を陽極として、液温１８℃、電流密度８Ａ／ｄｍ２で２１秒間電気めっき（銀めっき）を行って、基材上（の銀ストライクめっき皮膜上）に銀めっき皮膜を形成し、水洗して銀めっき液を十分に洗い流した。この銀めっき皮膜の幅方向略中央部の厚さを蛍光Ｘ線膜厚計（株式会社日立ハイテクサイエンス製のＳＦＴ－１１０Ａ）により測定したところ、１．０μｍであった。 Next, in the continuous plating line, silver plating consisting of an aqueous solution containing 175 g / L of silver potassium cyanide (KAg (CN) 2 ), 95 g / L of potassium cyanide (KCN) and 102 mg / L of potassium selenocyanate (KSeCN). In the liquid, the base material on which the silver strike plating film is formed is used as the cathode, and the silver particles housed in the titanium anode case are used as the anode, and electroplating (silver) at a liquid temperature of 18 ° C. and a current density of 8 A / dm 2 for 21 seconds. Plating) was performed to form a silver plating film on the substrate (on the silver strike plating film), which was then washed with water to thoroughly wash away the silver plating solution. The thickness of the silver-plated film at substantially the center in the width direction was measured by a fluorescent X-ray film thickness meter (SFT-110A manufactured by Hitachi High-Tech Science Corporation) and found to be 1.0 μm.
　次に、連続めっきラインにおいて、基材上の下地めっき皮膜からマスキングテープを剥がした後、基材の幅方向上端部から幅１５ｍｍの部分（銀めっき皮膜の全面と下地めっき皮膜の一部を覆う帯状部分）にマスキングテープを貼り付けた。 Next, in the continuous plating line, after removing the masking tape from the base plating film on the base material, the portion 15 mm wide from the upper end in the width direction of the base material (covering the entire surface of the silver plating film and a part of the base plating film). A masking tape was attached to the strip).
　次に、連続めっきラインにおいて、（金属錫塩として）アルカノールスルホン酸錫（ユケン工業株式会社製のメタスＳＭ－２）２５０ｍＬ／Ｌと（遊離酸として）アルカノールスルホン酸（ユケン工業株式会社製のメタスＡＭ）７５ｍＬ／Ｌとを含む錫めっき液中において、銀めっき皮膜を形成した基材を陰極とし、チタン製のアノードケースに収容された錫のボールを陽極として、液温２５℃、電流密度１２Ａ／ｄｍ２として１４秒間電気めっき（錫めっき）を行って、基材上のマスキングテープが貼られていない領域（基材上の下地めっき皮膜の露出面（被めっき材の幅方向下端部から幅１０ｍｍの領域））に厚さ１μｍの錫めっき皮膜を形成した後、マスキングテープを剥がした。 Next, in the continuous plating line, 250 mL / L of tin alkanolsulfonate (as metal tin salt) (Metas SM-2 manufactured by Yuken Kogyo Co., Ltd.) and alkanolsulfonic acid (metas manufactured by Yuken Kogyo Co., Ltd.) AM) In a tin plating solution containing 75 mL / L, the base material on which the silver plating film was formed was used as the cathode, and the tin balls housed in the titanium anode case were used as the anode, and the solution temperature was 25 ° C. and the current density was 12 A. Electroplating (tin plating) was performed for 14 seconds at / dm 2 , and the area on the base material where the masking tape was not attached (the exposed surface of the base plating film on the base material (width from the lower end in the width direction of the material to be plated). After forming a tin-plated film having a thickness of 1 μm in a 10 mm region)), the masking tape was peeled off.
　次に、錫めっき皮膜を形成した基材を、セラミックスパネルヒーターを用いた炉内に入れ、この炉内で予備加熱（この予備加熱では錫めっき皮膜は溶融していない）した後、平板面状放射型赤外線ランプ（アドバンス理工株式会社製のＰｓ１１０ＶＰ、単層２００Ｖ、２ｋＷ）に対向させて、出力６７％で１５秒間加熱することによりリフロー処理を行った。このリフロー処理により、錫めっき層が溶融した後に凝固し、リフロー錫めっき層が形成されていることが確認された。 Next, the base material on which the tin-plated film was formed was placed in a furnace using a ceramic panel heater, preheated in this furnace (the tin-plated film was not melted by this preheating), and then a flat plate surface was formed. The reflow treatment was performed by facing a radial infrared lamp (Ps110VP manufactured by Advance Riko Co., Ltd., single layer 200V, 2kW) and heating at an output of 67% for 15 seconds. It was confirmed that the tin plating layer was melted and then solidified by this reflow treatment to form the reflow tin plating layer.
　このようにして作製しためっき材について、リフロー処理の前後で銀めっき層の表面の接触抵抗を電気接点シミュレータ（株式会社山崎精機研究所製のＣＲＳ－１）により荷重１００ｇｆで測定したところ、リフロー処理前では０．７２ｍΩ、リフロー処理後では０．６４ｍΩであり、接触抵抗の上昇はなかった。また、銀めっき層の外観を目視で観察したところ、リフロー処理前後で変色は確認されなかった。 For the plating material produced in this way, the contact resistance on the surface of the silver plating layer was measured before and after the reflow treatment with an electric contact simulator (CRS-1 manufactured by Yamasaki Seiki Laboratory Co., Ltd.) under a load of 100 gf. It was 0.72 mΩ before and 0.64 mΩ after the reflow treatment, and there was no increase in contact resistance. Moreover, when the appearance of the silver-plated layer was visually observed, no discoloration was confirmed before and after the reflow treatment.
［比較例］
　錫めっき皮膜を形成した基材を、予備加熱した後に平板面状放射型赤外線ランプで加熱する代わりに、ホットプレート（アズワン株式会社製のＨＩＧＨ　ＴＥＭＰ　ＨＯＴＰＬＡＴＥ（型式ＨＴＨ－５００Ｎ））上に配置し、大気中において４５０℃で加熱した以外は、実施例と同様の方法により、めっき材を作製した。 [Comparison example]
Instead of preheating the base material on which the tin-plated film is formed and then heating it with a flat plate surface radiating infrared lamp, the base material is placed on a hot plate (HIGH TEMP HOTPLATE (model HTH-500N) manufactured by AS ONE Corporation). A plating material was prepared by the same method as in Examples except that the plating material was heated at 450 ° C. in the air.
　このようにして作製しためっき材について、実施例と同様の方法により、リフロー処理の前後で銀めっき層の表面の接触抵抗を測定したところ、リフロー処理前では０．７５ｍΩ、リフロー処理後では２．４９ｍΩであり、接触抵抗が大幅に上昇していた。また、銀めっき層の外観を目視で観察したところ、リフロー処理前後で変色が確認された。 When the contact resistance of the surface of the silver plating layer was measured before and after the reflow treatment of the plating material produced in this manner by the same method as in the example, 0.75 mΩ before the reflow treatment and 2. after the reflow treatment. It was 49 mΩ, and the contact resistance was significantly increased. Moreover, when the appearance of the silver-plated layer was visually observed, discoloration was confirmed before and after the reflow treatment.
　１０　基材
　１２　下地めっき皮膜（ニッケルめっき皮膜）
　１４　マスク部材
　１６　銀めっき皮膜
　１８　マスク部材
　２０　錫めっき皮膜
　２２　リフロー錫めっき層 10 Base material 12 Base plating film (nickel plating film)
14 Mask member 16 Silver plating film 18 Mask member 20 Tin plating film 22 Reflow tin plating layer

Claims (10)

  1. 銅または銅合金からなる基材の表面にニッケルめっき皮膜を形成し、このニッケルめっき皮膜の表面の一部に銀めっき皮膜を形成するとともに、ニッケルめっき皮膜の表面の他の部分の一部に錫めっき皮膜を形成することにより、基材上のニッケルめっき皮膜の表面に銀めっき皮膜と錫めっき皮膜が形成されためっき材を作製した後、このめっき材の表面に赤外線を照射して加熱することにより、錫めっき皮膜をリフロー処理して、錫めっき皮膜をリフロー錫めっき層にすることを特徴とする、めっき材の製造方法。 A nickel plating film is formed on the surface of a base material made of copper or a copper alloy, a silver plating film is formed on a part of the surface of the nickel plating film, and tin is formed on a part of the other part of the surface of the nickel plating film. By forming a plating film, a plating material in which a silver plating film and a tin plating film are formed on the surface of the nickel plating film on the base material is prepared, and then the surface of the plating material is irradiated with infrared rays and heated. A method for producing a plating material, which comprises reflowing a tin-plated film to form a reflowed tin-plated layer.
  2. 前記赤外線の照射の前に、前記ニッケルめっき皮膜の表面に銀めっき皮膜と錫めっき皮膜が形成されためっき材を、前記錫めっき皮膜が溶融しないように予備加熱することを特徴とする、請求項１に記載のめっき材の製造方法。 The claim is characterized in that, before the irradiation with infrared rays, a plating material having a silver plating film and a tin plating film formed on the surface of the nickel plating film is preheated so that the tin plating film does not melt. The method for producing a plating material according to 1.
  3. 前記赤外線の照射が、赤外線ランプにより行われることを特徴とする、請求項１に記載のめっき材の製造方法。 The method for producing a plating material according to claim 1, wherein the infrared irradiation is performed by an infrared lamp.
  4. 前記銀めっき皮膜を形成した後に前記錫めっき皮膜を形成することを特徴とする、請求項１に記載のめっき材の製造方法。 The method for producing a plating material according to claim 1, wherein the tin plating film is formed after the silver plating film is formed.
  5. 前記ニッケルめっき皮膜を形成した後、前記銀めっき皮膜を形成する前に、前記ニッケルめっき皮膜の表面の一部以外の部分をマスク部材によって覆うことを特徴とする、請求項４に記載のめっき材の製造方法。 The plating material according to claim 4, wherein a portion other than a part of the surface of the nickel plating film is covered with a mask member after the nickel plating film is formed and before the silver plating film is formed. Manufacturing method.
  6. 前記銀めっき皮膜を形成した後、前記錫めっき皮膜を形成する前に、前記ニッケルめっき皮膜の表面の他の部分の一部以外の部分と前記銀めっき皮膜の表面をマスク部材によって覆うことを特徴とする、請求項４に記載のめっき材の製造方法。 After forming the silver-plated film and before forming the tin-plated film, a mask member covers a portion other than a part of the surface of the nickel-plated film and the surface of the silver-plated film. The method for producing a plating material according to claim 4.
  7. 前記ニッケルめっき皮膜の表面の一部と、前記ニッケルめっき皮膜の表面の他の部分の一部が離間していることを特徴とする、請求項１に記載のめっき材の製造方法。 The method for producing a plating material according to claim 1, wherein a part of the surface of the nickel plating film and a part of the other part of the surface of the nickel plating film are separated from each other.
  8. 銅または銅合金からなる基材の表面にニッケルめっき層が形成され、このニッケルめっき層の表面の一部に銀めっき層が形成されているとともに、ニッケルめっき皮膜の表面の他の部分の一部にリフロー錫めっき層が形成され、銀めっき層の表面の接触抵抗が１ｍΩ以下であることを特徴とする、めっき材。 A nickel plating layer is formed on the surface of a base material made of copper or a copper alloy, a silver plating layer is formed on a part of the surface of the nickel plating layer, and a part of the other part of the surface of the nickel plating film. A plating material characterized in that a reflow tin plating layer is formed on the surface of the silver plating layer, and the contact resistance of the surface of the silver plating layer is 1 mΩ or less.
  9. 前記ニッケルめっき層の表面に形成されている前記銀めっき層と前記リフロー錫めっき層が離間していることを特徴とする、請求項８に記載のめっき材。 The plating material according to claim 8, wherein the silver plating layer formed on the surface of the nickel plating layer and the reflow tin plating layer are separated from each other.
  10. 請求項８に記載の銀めっき材を材料として用いたことを特徴とする、接点または端子部品。
          A contact or terminal component using the silver-plated material according to claim 8 as a material.
PCT/JP2020/002032 2019-03-29 2020-01-22 Plated material and method for manufacturing same WO2020202718A1 (en)

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